Dry size compositions



.Patented May 1946 UN [TED STATES PATENT OFFICE 2,401,090 a V i DRY SIZE COMPOSITIONS Robert T. Mashburn, Parchment; Mich, assignor to Hercules Powder Company, Wilmington, DeL, I a corporation of Delaware No Drawing. Application June 14, 1941,

Serial No. 398,024

9 Claims. (Cl. 106-144) 0 This invention relates to sizing compositions,

and in' particular concerns dry rosin size com- Although the paper-making art has for'many years in the past employed aqueoussolutions or dispersions'of saponified rosin almost exclusively for sizing purposes, with theacceptance-in re-; cent years of the so-called free rosin theory" ofsizing it has been realized that improved sizing efii'ciency and substantial 'manufacturing. economies= could be realized by the use of rosin size,

dispersions in which a high proportion of the rosin, e, g., 70-100 per cent, is present in free,

i. e., unsaponified, form. r

Accordingly, a number of sizing compositions of this'general .type have been proposed, and while several of such compositions have enjoyed 1 about per "cent; preferably between about 3 x and about 10 per cent, by weight of the rosin,.

although somewhat larger proportions may be moderate commercial usage, they have certain disadvantages which limit their general acceptance throughout the paper-making art. For example, it has been proposed in U. S. Patent No. 1,882,680

to prepare high free rosin size dispersions by agi-" tating molten rosin with an aqueous alkaline solution of a protective colloid such as casein.

Such dispersions, however, have the great disadvantage of being entirely unstable to freezing,-

refined wood or-gum rosin, or it'may' be a mixture of gum and wood rosins, Alternatively, it may be a rosin which has been subjected to heattreatment to reduce its tendency to crystallize, or

5 it maybe arosin which has been hydrogenated to renderit stableto discoloration or oxidationin theair. .v t.

The protective colloid employed ispreferably a proteinaceou material, such as milk casein, egg

1'0 albumin, soyabeantprotein, etc.,a1though other colloidal substancesysuchas gum arabic, starch,

water-soluble. methylcllulose, etc., may be em? ployed ifdesireda: Drysodium caseinate, such asis prepared.by .dissolving3milk casein in aqueous 15 sodium hydroxide and thereafter evaporating the resulting solution to dry fi has been found to be. particularly suitable because of its convenience in handling. The protective colloid is usually employed inamounts between about '1 and employed if desired. 0

The alkali'ingredientof the new dry size com- 28 positions is preferably=-an alkali-metal hydroxand accordingly. their shipment during winter tities of'water.

employed in anamount about 0.5 and between weather in northern climates becomes impossible. about 5 per cent by weight of the rosin, a is They have the further disadvantage in that they conveniently handled in the Iormofa concenare usuallyshipped at a solids concentration of trated aqueous solution.

about 40-50 percentby; weight, therebyneces- According to a preferred mode of preparing sitating the expense of transporting large quanthe dry-size compositions provided by the in- Y vention, the rosin is melted and the protective I have now found, that the aforementioned difficulties may be overcome by providing dry rosin sizev compositions "which are readily adapted to being-dispersed in'wate'r to form high free rosin size dispersions just prior to use in the paper mill. More specifically, I have found that a fused mixture of rosin, a protective colloid, and a small proportion of a water-soluble alkali may be readily dispersed in water with, the aid of an emcient stirring device to form high free rosin dispersions which are at least equal in sizing efllciency to the, sizing dispersions of this type pre-. viously employed and have excellent stability to i floccing upon dilution with hard water. Such dry mixture is entirely unaffected by exposure to freezing temperatures and is more economical to ship by reason of its being substantially free from water.

The rosin employed in preparing the new dry size compositions may be any or the grades of 40 broken up and packaged in the same manner as rosin. It is entirely stable to decomposition'or degradation .upon storageat atmospheric temperatures over long periods of time.

, As hereinbefore stated. the dry-size composttions of the present invention are readily dispersed in water to form aqueous sizing-dispersions adapted tobeing added directly to the beating engine in the paper-making process.

The dispersing operation may be carried out simply by melting the dry material and thereafter gradually adding the desired amount of water to vthe molten mass with vigorous agitatlon, such as that provided by a high-speed propeller-t pe agitator. iThe solids concentration of the dispersions so prepared may be varied be- Example Approximately 100 parts of refined wood rosin were placed in a kettle and melted by heating to a temperature of about 100 C., after which a solution of 1.8 parts of sodium hydroxide in 3.6

parts of water, and parts of dry sodium case- 1 inate were stirred into the molten rosin. Stirring was continued for several minutes to insure a homogeneous composition and the mixture was then allowed to cool. The composition so prepared was a hard, brittle material having the general appearance and color of rosin. A typical size dispersion was prepared from this material by melting it and thereafter gradually adding 118 parts of water while stirring with a high speed propeller-type stirrer. The resulting dispersion contained approximately 46.3 per cent by weight of solids, and approximately 85 per cent by weight of the rosin was present in free form as determined by direct titration.

The following table presents data illustrating the sizing efficiency of the above-described dispersion in comparison with that of several typical commercial dispersions. In the table, the data in Experiments 1 and 2 were obtained employing a beater furnish comprising 750 pounds of bleached sulflte pulp and 750 pounds of washed stock, and employing suflicient of the sizing dispersion to provide 19.4 pounds of rosin. The sizing dispersion wasadded to the beater, after which suflicient alum was added to maintain a' 9 pH of about 4.0-4.3, and the sized furnish was run off on a Fourdrinier machine at a rate of about 235 feet per minute. After drying and conditioning, samples of the paper so prepared were subjected to the tests indicated in the table. The data in Experiments 3 and 4 were obtained with a somewhat different beater furnish. All of the values in said table represent the average of separate determinations on at least four separate samples of the paper.

homogeneous mixture consisting essentially of molten rosin, a wateror alkali-soluble protective colloid, and between about 0.5% and about 1% by weight ofthe rosin of a water-soluble alkali metal alkali, said product being a. hard, brittle material having the general appearance and color of rosin and being stable to decomposition and degradation upon storage over long periods of time; 4

2. A dry rosin size composition readily dispersible in water to provide an aqueous sizing dispersion. containing a high proportion of free rosin, comprising the solidified product of a homogeneous mixture consisting essentially of 5 molten rosin, a protective proteinaceous colloid,

and between about 0.5% and about 5% by weight of the rosin of a water-soluble alkali metal alkali, said product being a hard, brittle material having the general appearance and color of rosin and being stable to decomposition and degradation upon storage over long Iperiods of time.

3. A dry rosin size composition readily dispersible in water to provide an aqueous sizing dispersion containing a high proportion of free rosin, comprising the solidified product of a homogeneous mixture consisting essentially of molten rosin, a wateror alkali-soluble protective colloid, and between about 0.5% and about 5% by weight of the rosin of sodium hydroxide, said product being a hard, brittle material having the general appearance and color of rosin and bein stable to decomposition and degradation upon storage over long periods of time.

' 4. A dry rosin size composition readily dispersible in water to provide an aqueous sizing dispersion containing a high proportion of free rosin, comprising the solidified product of a homogeneous mixture consisting essentially of molten rosin, between about 1% and about 25% by weight of the rosin of ,a wateror alkali-soluble protective colloid and between about 0.5% and about 5% by weight of the rosin of a watersoluble alkali metal alkali, said product being a hard, brittle material having the general appearance and color of rosin and being stable to decomposition and degradation upon storage over long periods of time.

5. A dry rosin size composition readily dis- Table Basis weight. Gurley den- Ink flot- Water g Size dispersion lbs. (500 24 x someter poation, i penetra- 36 sheets) rosity, secs. secs. tion, secs.

rep red as herein described e0. 0 22. 5 310 6 a Commercial paste size containing 25% free rosin. 69. 9 22. l 197 7 l repared as herein described i 31. c 93. 14. 4 m ercial high free rosin size dispersion i 31. 4 s7 14. 0

l 480 24 x 36 Sheets.

Other modes of applying the principle of my invention may be employed insteadoi' those explained, change being made as regards the method herein disclosed or the materials employed, provided the product stated by any of the following claims or the equivalent of such stated product be obtained.

, What I claim and desire to protect by Letters Patent is:

l. A dry rosin size composition readily dispersible in .water to provide an aqueous sizing dispersion containing 9, high proportion of free rosin, comprising the solidified product of a homogeneous mixture by weight of the rosin between about 0.5%

ing aha'rd, brittle appearance and color of consisting essentially of about 1% and about 25% of sodiumcaseinate, and

molten rosin, between metal salt of soybean protein, and between about 0.5% and about 5% by weight of therosin of a water-soluble alkali metal alkali, said product being ahard, brittle material having the general appearance and color of rosin and being stable to decomposition and degradation upon storage over long periods of time.

8. A dry rosin size composition readily dispersible, in water to provide an aqueous sizing and about 5% by weight of rosin, comprising the s homogeneous mixture consisting essentially of molten. rosin, a water-soluble protective colloid,

and between about 0.5% and about 5% by'weight of the rosin of sodium appearance and colorof decomposition and degradation upon storage over long periods of time.

9. A dry rosin size composition readily dis persible in water to dispersion containing provide an aqueous sizing rosin, comprising the solidified product of a I by weight of therosin homogeneous mixture consisting essentially'of molten rosin, between about 3% and about 10% of sodium caseinate,and between about 0.5% and about 5% by weight "of the rosin of sodium hydroxide, said product being a hard, brittle material having the general appearance and color of rosin and being stable to decomposition and degradation upon storage over long periods of time.

ROBERT 'r. MASHBURN.

dispersion containing a high proportion ofire lidifled product ,of a

carbonate, said product. being a. hard, brittle material having the general rosin and being stable to a high proportion of free 

